HRID1707003

反应详情

EQUATION

反应方程式

HRID 1707003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5.02 g (0.02 mole) of (2-chloroacetamido)-malonic acid diethyl ester [see Ajay Kumar Bose, J.Indian Chem. Soc. 31, 108-110 (1954)] and 4.50 g (0.03 mole) of sodium iodide in 100 ml of acetone is refluxed for 30 minutes. The reaction mixture is thereupon concentrated in vacuo. Water is added to the residue, and extraction is performed twice with methylene chloride. The organic phase is washed once with diluted aqueous sodium bisulphite solution and twice with saturated sodium chloride solution; it is dried over sodium sulphate and concentrated in vacuo. The residue is recrystallised from methylene chloride/hexane. After filtration with suction and drying in vacuo, there is obtained (2-iodoacetamido)-malonic acid diethyl ester, m.p. 95°-97°.

WORKUP

后处理

  1. concentrationThe reaction mixture is thereupon concentrated in vacuo
  2. additionWater is added to the residue, and extraction
  3. washThe organic phase is washed once with diluted aqueous sodium bisulphite solution and twice with saturated sodium chloride solution
  4. dry with materialit is dried over sodium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe residue is recrystallised from methylene chloride/hexane
  7. filtrationAfter filtration with suction
  8. customdrying in vacuo